Development of a three-steps derivatization assay for the localization of double bond in monounsaturated monomers of poly-beta-hydroxyalkanoates by GC-MS

作者：Simon Colin Christelle^*; Gouin Christelle; Lemechko Pierre; Kervarec Nelly; Guezennec Jean

来源：Journal of Chromatography B-Analytical Technologies in the Biomedical and Life Sciences, 2012, 900: 64-70.

DOI：10.1016/j.jchromb.2012.05.032

• Poly-beta-hydroxyalkanoate
• Unsaturation
• DMDS derivatives
• Acetylation
• GC-MS

A new gas chromatography-mass spectrometry (GC-MS) method for the localization of double bond in monounsaturated 3-hydroxyalkenoic acids monomers has been developed. A three steps derivation assay was used including a methanolysis, then acetylation and dimethyldisulfide (DMDS) addition to alkene groups. Electron impact GC-MS analysis of such derivatives offers characteristic fragments allowing the unambiguous determination of double bond position in side chain. This novel method is well-suited for the routine analysis of poly-beta-hydroxyalkanoates (PHAs), and was used to characterize monounsaturated monomers in both 3-hydroxyalkenoic acids standards as well as in mcl-PHAs and poly(3-hydroxyoctanoate-co-3-hydroxyundecenoate) (PHOU) produced by bacterial strain Pseudomonas guezennei from glucose or a mixture of sodium octanoate plus 10-undecenoic acid, respectively.

• 出版日期2012-7-1